CN109761620A - A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride - Google Patents
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride Download PDFInfo
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- CN109761620A CN109761620A CN201910163436.5A CN201910163436A CN109761620A CN 109761620 A CN109761620 A CN 109761620A CN 201910163436 A CN201910163436 A CN 201910163436A CN 109761620 A CN109761620 A CN 109761620A
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Abstract
The invention discloses a kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, include the following steps: 1) to weigh α-Si by predetermined ratio3N4、CeO2、Y2O3Powder carries out ball milling mixing；2) mixed powder after ball milling is dried, and be sieved；3) powder screened is subjected to precompressed；4) under vacuum or argon atmosphere, the discharge plasma sintering combined using electric current heating and radiant heating, sintering temperature is 1600-1700 DEG C, keeps the temperature 0-5min to get the compact silicon nitride is arrived.Present invention process is simple, sintering time is short, sintering temperature can be greatly reduced, and increase radiation heater, and it is mounted with insulating layer, by adjusting additional thermal power and main heating power match parameter, the uniformity in mould inside temperature field is improved, to provide effective guarantee to be sintered the large-scale silicon nitride ceramics of even compact.
Description
Technical field
The invention belongs to discharge plasma sintering field of material technology, and in particular to a kind of dual heating mode plasma discharging
The method that sintering prepares compact silicon nitride.
Background technique
Silicon nitride ceramics is wear-resistant due to anti-oxidant, and corrosion resistance is good, and fracture toughness is high, and specific gravity is small, thermal conductivity height etc.
Advantage occupies an important position in new ceramics, is a kind of ideal high-speed cutting tool ceramics material.With other ceramic phase ratios,
For silicon nitride ceramics since its thermal expansion coefficient is small, thermal shock resistance is good, and fracture toughness is high, and specific gravity is small, and thermal conductivity is high, under high temperature
Hardness and intensity it is high, the advantages that creep is small, also often as high-temperature structural material, is widely used in machinery, chemical industry, ocean work
The key areas such as journey, aerospace.
The sintering of silicon nitride ceramics at this stage is mainly passed by no pressure, hot pressing, air pressure, hot isostatic pressing, reaction-sintered etc.
Based on system sintering processing, but because the drawbacks such as conventional sintering mode energy consumption height, sintering time length, low efficiency greatly limit Si3N4Pottery
The large-scale production of porcelain.Discharge plasma sintering can apply certain mechanical force during Fast Sintering, be easy to get cause
Close block materials, be it is a kind of quickly, low temperature, energy-saving and environmental protection material preparation New Machining Technology, have sintering quickly, sintering
The advantages that temperature is low, sintering mechanism is special, simple to operate, and make final product have fine microstructures uniformly, can protect
Hold the nature of raw material, the features such as consistency is high, but the block that more and more user's discoveries are prepared using this method
When material diameter is greater than 30mm, the non-uniform phenomenon of internal structure would generally inevitably occur in sample.
Summary of the invention
The present invention provides a kind of fine and close nitridation of dual heating mode discharge plasma sintering preparation to solve above-mentioned technical problem
The method of silicon.This method can be sintered out material internal uniformly densely silicon nitride ceramics.
Realize that the technical solution of above-mentioned purpose is as follows:
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, includes the following steps:
1) α-Si is weighed by predetermined ratio3N4、CeO2、Y2O3Powder carries out ball milling mixing；
2) mixed powder after ball milling is dried, and be sieved；
3) powder screened is subjected to precompressed；
4) under vacuum or argon atmosphere, the discharge plasma sintering combined using electric current heating and radiant heating,
Sintering temperature is 1600-1700 DEG C, keeps the temperature 0-5min to get the compact silicon nitride is arrived.
In above scheme, the power of radiant heating is 30-80kWh, and the power of electric current heating is 40-100kWh.
In above scheme, during the discharge plasma sintering of electric current heating and radiant heating combination, radiant heating is first opened
System opens simultaneously electric current heating system when sample is heated to 300-800 DEG C.
In above scheme, each component is calculated in mass percent as follows in step 1): α-Si3N495-98%, CeO2 1-
4%, Y2O31-4%.
In above scheme, ball milling mixing described in step 1) is that weighed powder is put into ball grinder, with anhydrous second
Alcohol is medium.
In above scheme, ball grinder described in step 1) is polytetrafluoroethylene (PTFE) ball grinder, and abrading-ball selects agate ball, ball material
Than for 3:1.
In above scheme, the ball milling mixing time is 12-24h in step 1).
In above scheme, the powder screened is placed in the circular graphitic mold that internal diameter is 50mm in step 3), precompressed
Time 1-2min is pressed under the pressure of 10MPa in advance and carries out.
In above scheme, the pressure applied in step 4) sample sintering process is 30-50MPa.
It is used to set in the discharge plasma sintering process that electric current heating adopted by the present invention and radiant heating combine
It is standby as shown in Figure 1.The equipment includes sample 1, sintering graphite mold 2,3 ﹑ sintering furnace body 4 of radiating heat element and high temperature insulating
Body 5.Sintered sample 1 is placed on inside sintering graphite mold, electric current by 1 inside of graphite jig 2 or sample (when conductivity compared with
Gao Shi, electric current simultaneously flow through graphite jig and sample interior；When being sintered non-conducting material, electric current flows mainly through mold) to sample
Product carry out electric current heating.Radiating heat element 3 is radiant heating heater, and 5 be high temperature insulating layer, radiates sintered component 3 to sample
Product carry out radiant heating.Radiant heating fever volume morphing can install shape etc., and radiant heating for circle cylinder shape ﹑ square tube shape ﹑ dispersion
Heater is graphite using material.Thermal insulation layer material is carbon fiber felt.Thermal insulation layer can reduce the outside heat consumption of die surface
It dissipates.The present invention is exactly the dual heating mode flash sintering method for taking electric current heating to combine radiant heating, in traditional electric discharge
A set of radiant heating device is added on the basis of plasma agglomeration.It is same using electric current heating and two kinds of heating modes of radiant heating
When the composite heating mode that works, the advantages of it inherits discharge plasma sintering (heating rate is fast), changed simultaneously sintering
Temperature distributing rule in the process realizes the dense samples of the uniform larger size of preparation structure, and sintering time Duan ﹑ is saved
Energy.Had a definite purpose using two sets of heating modes: electric current heating can be achieved to be rapidly heated, and samming then can be achieved in radiant heating, change
Radial temperature profile in kind sintered sample and mold obtains uniform temperature especially in the radial temperature profile of sample interior
Field is spent, is effectively ensured to be provided for the uniform block materials of preparation structure.
The present invention has the advantage that
(1) heating rate is very fast, and sintering time shortens, and improves production efficiency, is easy to large-scale production；
(2) sintering temperature of silicon nitride ceramics can be significantly reduced；
(3) by adjusting the radiant heating power match parameter of main electric current heating power and auxiliary, mold table can be made
Within temperature difference control 15% between face temperature and radiation heater, guarantee the consistency of sample interior temperature, thus for preparation
The large-scale silicon nitride ceramics of even compact provide effective guarantee.
Detailed description of the invention
Fig. 1 to realize the present invention method with radiation heat generating device electric current sintering system structural schematic diagram.
In figure: 1- sample, 2- mold, 3- radiant heating heater, 4- sintering furnace body, 5- high temperature insulating layer.
Fig. 2 is the SEM figure of the fracture surface of silicon nitride ceramic material made from embodiment 1.
Fig. 3 is the SEM figure of the fracture surface of silicon nitride ceramic material made from embodiment 3.
Fig. 4 is the SEM figure of the fracture surface of silicon nitride ceramic material made from embodiment 6.
Specific embodiment
Below by way of drawings and examples, the present invention will be described in detail.
Embodiment 1
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, specifically: by weight percent
Weigh α-Si3N495%, CeO21%, Y2O34% carries out ingredient, by the mixed powder matched using dehydrated alcohol as medium, Ma
Nao ball is abrading-ball, is put into polytetrafluoroethylene (PTFE) ball grinder ball milling for 24 hours, ratio of grinding media to material 3:1；It is dried after ball milling, and crosses 200 meshes,
Powder after sieving is placed in the circular graphitic mold that internal diameter is 50mm and carries out precompressed, pressure 10MPa, pressure maintaining 2min；It will
Graphite jig is put into the chamber of dual heating mode discharge plasma sintering system, and vacuum degree is 6Pa or less in furnace chamber；Apply pressure
Power 50MPa, unlatching sintering button is heated, and with additional thermal power 30kWh heating, when temperature reaches 300 DEG C, opens main add
Hot systems, main heating power are 80kWh, and sample is heated to 1600 DEG C, keeps the temperature 5min, then furnace cooling.After tested,
The consistency of material is 98.72%.It is scanned electron microscope (SEM) (Fig. 2) analysis, material internal is uniformly closely knit, uses
This dual heating mode discharge plasma sintering method has prepared structure uniformly closely knit block materials.
Embodiment 2
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, specifically: by weight percent
Weigh α-Si3N495%, CeO24%, Y2O31% carries out ingredient, by the mixed powder matched using dehydrated alcohol as medium, Ma
Nao ball is abrading-ball, is put into polytetrafluoroethylene (PTFE) ball grinder ball milling for 24 hours, ratio of grinding media to material 3:1；It is dried after ball milling, and crosses 200 meshes,
Powder after sieving is placed in the circular graphitic mold that internal diameter is 50mm and carries out precompressed, pressure 10MPa, pressure maintaining 1min；It will
Graphite jig is put into the chamber of dual heating mode discharge plasma sintering system, and vacuum degree is 6Pa or less in furnace chamber；Apply pressure
Power 30MPa, unlatching sintering button is heated, and with additional thermal power 70kWh heating, when temperature reaches 400 DEG C, opens main add
Hot systems, main heating power are 40kWh, and sample is heated to 1600 DEG C, keeps the temperature 5min, then furnace cooling.After tested,
The consistency of material is 97.93%
Embodiment 3
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, specifically: by weight percent
Weigh α-Si3N495%, CeO24%, Y2O31% carries out ingredient, by the mixed powder matched using dehydrated alcohol as medium, Ma
Nao ball is abrading-ball, is put into ball milling 12h in polytetrafluoroethylene (PTFE) ball grinder, ratio of grinding media to material 3:1；It is dried after ball milling, and crosses 200 meshes,
Powder after sieving is placed in the circular graphitic mold that internal diameter is 50mm and carries out precompressed, pressure 10MPa, pressure maintaining 1 minute；It will
Graphite jig is put into the chamber of dual heating mode discharge plasma sintering system, by vacuum state in furnace chamber；Apply pressure
Power 70MPa, unlatching sintering button is heated, and with additional thermal power 70kWh heating, when temperature reaches 600 DEG C, opens main add
Hot systems, main heating power are 80kWh, and sample is heated to 1700 DEG C, keeps the temperature 5min, then furnace cooling.After tested,
The consistency of material is 98.32%.It is scanned electron microscope (SEM) (Fig. 3) analysis, material internal is uniformly closely knit, helps burning
Knot agent is wrapped in silicon nitride grain surface in the form of vitreum, is prepared using this dual heating mode discharge plasma sintering method
Structure uniformly closely knit block materials are gone out.
Embodiment 4
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, specifically: by weight percent
Weigh α-Si3N495%, CeO22%, Y2O33% carries out ingredient, by the mixed powder matched using dehydrated alcohol as medium, Ma
Nao ball is abrading-ball, is put into ball milling 16h in polytetrafluoroethylene (PTFE) ball grinder, ratio of grinding media to material 3:1；It is dried after ball milling, and crosses 200 meshes,
Powder after sieving is placed in the circular graphitic mold that internal diameter is 50mm and carries out precompressed, pressure 10MPa, pressure maintaining 1 minute；It will
Graphite jig is put into the chamber of dual heating mode discharge plasma sintering system, by vacuum state in furnace chamber；Apply pressure
Power 50MPa, unlatching sintering button is heated, and with additional thermal power 50kWh heating, when temperature reaches 800 DEG C, opens main add
Hot systems, main heating power are 60kWh, and sample is heated to 1600 DEG C, keeps the temperature 3min, then furnace cooling.After tested,
The consistency of material is 99.94%.
Embodiment 5
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, specifically: by weight percent
Weigh α-Si3N498%, CeO21%, Y2O31% carries out ingredient, by the mixed powder matched using dehydrated alcohol as medium, Ma
Nao ball is abrading-ball, is put into polytetrafluoroethylene (PTFE) ball grinder ball milling for 24 hours, ratio of grinding media to material 3:1；It is dried after ball milling, and crosses 200 meshes,
Powder after sieving is placed in the circular graphitic mold that internal diameter is 50mm and carries out precompressed, pressure 10MPa, pressure maintaining 1 minute；It will
Graphite jig is put into the chamber of dual heating mode discharge plasma sintering system, by vacuum state in furnace chamber；Apply pressure
Power 50MPa, unlatching sintering button is heated, and with additional thermal power 60kWh heating, when temperature reaches 700 DEG C, opens main add
Hot systems, main heating power are 50kWh, and sample is heated to 1650 DEG C, without heat preservation, then furnace cooling.After tested
, the consistency of material is 96.50%.
Embodiment 6
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, specifically: by weight percent
Weigh α-Si3N496%, CeO22%, Y2O32% carries out ingredient, by the mixed powder matched using dehydrated alcohol as medium, Ma
Nao ball is abrading-ball, is put into ball milling 18h in polytetrafluoroethylene (PTFE) ball grinder, ratio of grinding media to material 3:1；It is dried after ball milling, and crosses 200 meshes,
Powder after sieving is placed in the circular graphitic mold that internal diameter is 50mm and carries out precompressed, pressure 10MPa, pressure maintaining 1 minute；It will
Graphite jig is put into the chamber of dual heating mode discharge plasma sintering system, by vacuum state in furnace chamber；Apply pressure
Power 60MPa, unlatching sintering button is heated, and with additional thermal power 30kWh heating, when temperature reaches 400 DEG C, opens main add
Hot systems, main heating power are 70kWh, and sample is heated to 1620 DEG C, without heat preservation, then furnace cooling.After tested
, the consistency of material is 98.74%.It is scanned electron microscope (SEM) (Fig. 4) analysis, material internal is uniformly closely knit, adopts
Structure uniformly closely knit block materials have been prepared with this dual heating mode discharge plasma sintering method.
Embodiment 7
A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, specifically: by weight percent
Weigh α-Si3N495%, CeO21%, Y2O34% carries out ingredient, by the mixed powder matched using dehydrated alcohol as medium, Ma
Nao ball is abrading-ball, is put into polytetrafluoroethylene (PTFE) ball grinder ball milling for 24 hours, ratio of grinding media to material 3:1；It is dried after ball milling, and crosses 200 meshes,
Powder after sieving is placed in the circular graphitic mold that internal diameter is 50mm and carries out precompressed, pressure 10MPa, pressure maintaining 1 minute；It will
Graphite jig is put into the chamber of dual heating mode discharge plasma sintering system, by vacuum state in furnace chamber；Apply pressure
Power 40MPa, unlatching sintering button is heated, and with additional thermal power 40kWh heating, when temperature reaches 600 DEG C, opens main add
Hot systems, main heating power are 70kWh, and sample is heated to 1600 DEG C, without heat preservation, then furnace cooling.After tested
, the consistency of material is 97.36%.
Claims (9)
1. a kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride, which is characterized in that including walking as follows
It is rapid:
1) α-Si is weighed by predetermined ratio3N4、CeO2、Y2O3Powder carries out ball milling mixing；
2) mixed powder after ball milling is dried, and be sieved；
3) powder screened is subjected to precompressed；
4) under vacuum or argon atmosphere, the discharge plasma sintering combined using electric current heating and radiant heating, sintering
Temperature is 1600-1700 DEG C, keeps the temperature 0-5min to get the compact silicon nitride is arrived.
2. the method as described in claim 1, which is characterized in that the power of radiant heating is 30-80kWh, electric current heating
Power is 40-100kWh.
3. the method as described in claim 1, which is characterized in that the discharge plasma sintering of electric current heating and radiant heating combination
In the process, radiating heat system is first opened, electric current heating system is opened simultaneously when sample is heated to 300-800 DEG C.
4. the method as described in claim 1, which is characterized in that each component is calculated in mass percent as follows in step 1): α-
Si3N495-98%, CeO21-4%, Y2O31-4%.
5. the method as described in claim 1, which is characterized in that ball milling mixing described in step 1) is to put weighed powder
Enter in ball grinder, using dehydrated alcohol as medium.
6. the method as described in claim 1, which is characterized in that ball grinder described in step 1) is polytetrafluoroethylene (PTFE) ball milling
Tank, abrading-ball select agate ball, ratio of grinding media to material 3:1.
7. the method as described in claim 1, which is characterized in that the ball milling mixing time is 12-24h in step 1).
8. the method as described in claim 1, which is characterized in that it is 50mm's that the powder screened, which is placed on internal diameter, in step 3)
In circular graphitic mold, squeeze time 1-2min is pressed under the pressure of 10MPa in advance and carries out.
9. the method as described in claim 1, which is characterized in that the pressure applied in step 4) sample sintering process is 30-
50MPa。
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